Process of producing brown shades on fiber.



UNITED STATEs 'PATENT oFFroE.

HENRI SCHED, OF MLHAUSEN. GERMANY, ASSIGNOB. TO BADISCHE ANILIN 6530EA Fm, 0F LUD'WIGSHAFEN-0N-THELRHINEi GERMANY, A COREORATION.

PROCESS F PRODGING BEK-OWN SHADES 03 FIBER.

lo Dravingpeccation of Letters Patent.

resented Apr, '1, 1914.

Application filed December S, 1912. Serial No, 734,55'.

f Wn that I, HENRI Soriano, citizen of the 'iss Republic` residing :it Mlhausen, Germany, have invented new und use-ful Improvements in Processes of Producing Brown Shades on Fiber, ot' which the following is u specification.

I have found that valuable and fast brown shades can be obtained on ber in a simple manner by the oxidation, by means of n chlorate, of orthddianisidin dissolved in acid. In order to avoid damaging the fiber, it is preferred to use solution ot' orthodianisidin in an orgunic arid, or in a miie ture of an organic arid with u -coinparatirely small quantity of mineral acid, for instance n quantity of mineral seid Cun be used'whieh would only suffise to' Combine completely with one-fourth the quantity of base employed.

The use of n vanadium salt to assist in the reaction, as is usual in the prodiuiion of K yanilin black, is not suitable for the purposes of my invention, because the vanadium salts act too energeticallynnd cause n too rapid oxidation both of the beth and of the mn.- terial which has beenv padded, so that. on steaming the material. only s light brown shade is obtained linstead of n full dark brown shade. lt is, however. often advisable to promote the reaction by means of suitable catalyzers7 as then the ortho-dimisi .din is used up to the greatest adrnntage and a quick and certain action is insure l. As instances, of such cntalyzers. l mention me tallic silts which react less energetically than vanadium salts and in particular iron salts and copper salts. As rule. as small quantities as possible of these salts should be employed so as to prevent oxidation taki place too soon hen preparing the pudding or printing mixtures, the additions usual in such operations, such for instance es neet-in. can be made. Also potassium ferrocyanid can be added and the peculiar et'ert is obtained that the shade varies ncordiug to the quantity of potassium ferroeyanid employed; for e ample, by Suitable variation of the quantityv em loyed, verz@7 bright and light orange to radi-)brown shades of excellentl tesine-ss can be obtained, or bright yellow-brown. orangebrown, or old gold. or rust;T brown. or chamois, shades can be produfed. ln eonsequnce of this action of the ferrotjvanid. putterne un be obtained by printing pastas containing potassium ferrocyanid on materiel which already padded with the diallisidin nurture und then steaming the goods. Other variations Cnn he obtained by printing a chloride mixture, which muy be of the usual kind generally employe-l for discharging coloring matters from fiber, on material which yhss already been developed either with or without white reserve effects. Qn 61' stunning the material thus printeibeeutb tul golden yellow .patterns on e brown ground are obtained. Dianisidin can be thus employed for the production of a very greet number or' different shades, such as hitherto 7C could not be obtained by the oxidation of one und the seme amin. In the case of all the shades obtained in the aforesaid manner,

the material run be reserved either White or in colors by treating, with a reducing 'le ugent, the padded or printed materia-l betore stesmin.

the E llowing example wili serve to illustrate further the nature of my invention, wliiob, hou-ever, is not confined to this ex- Se ample. The paris are by weight: Prepare a padding liquor in the following manner: Dissolve 28 psrtsof ortho-dianisidin in 7 parte ot 30% hydoclorio acid and from 18 to Q0 ports of 90% fornxic scid and s little iva-ter. 'While warming. 1When the solution is cold. add a solution of 25 parts of sodium chlomte dissolved in a little water and make up the whole with water to L00() parts. As :t cntalyzer from 0.5 to 0.75 part Aof ferrous so sul-tate or potassium ferrocya'nid can be added. Pad the material Wit this solution, dry, nndstearn in a lvlather-Platt ap sratus. A manganese bronze shade is thus ovtained. lt trfu'u l() to 30 parts of potassium ferroe5 cyzmid be added to the padding bath, a brighter brownish orange shade is produced.

To produce a printing paste, the usual or any suitable thielrenings and other suitable ugents can be added.

Now what l Claim ierl. The process of producing brown shades on fiber by applying to the material orthodianisidin sind less than one equivalent of mineral unid for each equivalent of orthodifini '.din employed and a chlorate, and then Causing the oxidation of the ortho-dianisidin substantially as hereinbefore described.

The process of producing brown shades on tiberby applying to the material ortho- 11C dianisidin and less than one equivalentof mineral acid for each equivalent of orthodianisidin` employed and a chlorate and a suitable cata-lyzer, and then causing the oxidation of the ortho-dianisidin` substantially as hereinbefore described.

3. The process of producing brown shades on fiber by applying to the material orthodianisidin andless than one equivalent of mineral acid for each equivalent of ortlif dianisidin employed and a clilorate and a small quantity of potassium errocyanid, and then causing the oxidation of the orthodianisidin substantially as hereinbefore described.

4i The process of producing brown shades on-iber by applying to the material orthodianisidin, an organic acid, a quantity of inorganic acid suicient to combine with about one-fourth of the quantity of baseernployed, and alkali metal chlorate, and then causing the oxidation of the ortho-dianisidin.

5. The. process of producing brown shades on fiber by applying to the material orthodianisidin and less than one equivalent of mineral acid foreach equivalent of orthodianisidi'n employed and a chlorate, and then subjecting the material to the action of steam.

6. The process of producing brown shades on fiber by applying to the material orthc dianisidin and less than one equi `lent of mineral acid for each equivalent ol' orthodianisidin employed and a. chlorate and a suitable catalyzer, and then subjecting the with a reducing agent and subjecting it to'- the action of steam.

8. The process of producing brown shades with reserve elle-cts on ber by applying to the material ortho-dianisidin and less than one equivalent of mineral acid Jfor each equivalent of ortho-dianisidin employed and a chlorate and a suitable catalyzer, and then treating the material with a reducing agent and subjecting it to the action of steam.

In testimony whereof I have hereunto seit, my hand in the presence of two subscribing witnesses.

HENRI SCHMID.

Witnesses GEO. Glrronn, ARNOLD Zonen. 

